Solvent-free, open-vessel microwave-promoted Heck couplings: From the mmol to the mol scale

Synlett

Volumn , Issue 18, 2006, Pages 2953-2958

  Leadbeater, Nicholas E ^a   Williams, Victoria A ^a   Barnard, Thomas M ^b   Collins Jr , Michael J ^b  

^a UNIVERSITY OF CONNECTICUT   (United States)

^b CEM Microwave Technology   (United States)

Author keywords

Catalysis; Heck reaction; Microwave; Palladium; Solvent free

Indexed keywords

4 IODOANISOLE; ACRYLIC ACID BUTYL ESTER; ACRYLIC ACID METHYL ESTER; IODINE DERIVATIVE; IODOBENZENE; PALLADIUM ACETATE; SODIUM CARBONATE; SOLVENT; TETRABUTYLAMMONIUM; TRIBUTYLAMINE; UNCLASSIFIED DRUG;

ARTICLE; CATALYST; CHEMICAL REACTION; CHEMICAL STRUCTURE; COUPLING FACTOR; MEDICAL INSTRUMENTATION; METHODOLOGY; MICROWAVE RADIATION; SCALE UP;

EID: 33751259643     PISSN: 09365214     EISSN: None     Source Type: Journal    
DOI: 10.1055/s-2006-951512     Document Type: Article

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70. (a) It is important that a suitably sized reaction vessel is used for scale-up reactions in the absence of solvent. It is advised that the contents should occupy no more than 10% of the vessel volume. In addition, microwave power should be carefully modulated. A power no greater than 600 W is advised.
71. (b) At a first glance it may seem that this would be putting in much more microwave power than in the case of the monomode experiments. However, the relative size of the cavity needs to be considered. Multimode microwaves have large cavities and so power is dissipated over a large area. Monomode equipment has a much smaller cavity and the energy density is up to some 30-40 times higher than the multimode apparatus.